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A green flow-based procedure for fluorimetric determination of acid-dissociable cyanide in natural waters exploiting multicommutation

机译:基于绿色流的多交换法荧光测定天然水中酸可分解的氰化物

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摘要

A flow system designed with solenoid valves is proposed for determination of weak acid dissociable cyanide, based on the reaction with o-phthalaldehyde (OPA) and glycine yielding a highly fluorescent isoindole derivative. The proposed procedure minimizes the main drawbacks related to the reference batch procedure, based on reaction with barbituric acid and pyridine followed by spectrophotometric detection, i.e., use of toxic reagents, high reagent consumption and waste generation, low sampling rate, and poor sensitivity. Retention of the sample zone was exploited to increase the conversion rate of the analyte with minimized sample dispersion. Linear response (r=0.999) was observed for cyanide concentrations in the range 1-200 mu g L-1, with a detection limit (99.7% confidence level) of 0.5 mu g L-1(19 nmol L-1). The sampling rate and coefficient of variation (n=10) were estimated as 22 measurements per hour and 1.4%, respectively. The results of determination of weak acid dissociable cyanide in natural water samples were in agreement with those achieved by the batch reference procedure at the 95% confidence level. Additionally to the improvement in the analytical features in comparison with those of the flow system with continuous reagent addition (sensitivity and sampling rate 90 and 83% higher, respectively), the consumption of OPA was 230-fold lower.
机译:基于与邻苯二甲醛(OPA)和甘氨酸的反应生成高荧光异吲哚衍生物,提出了一种设计有电磁阀的流动系统,用于测定弱酸可分解的氰化物。基于与巴比妥酸和吡啶的反应,然后分光光度检测,即使用有毒试剂,试剂消耗和废物产生高,采样率低,灵敏度低,拟议的程序将与参考批处理程序有关的主要缺点减至最小。利用保留样品区域来提高样品分散度最小的分析物的转化率。氰化物浓度在1-200μg L-1范围内观察到线性响应(r = 0.999),检出限(99.7%置信水平)为0.5μg L-1(19 nmol L-1)。采样率和变异系数(n = 10)分别估计为每小时22次测量和1.4%。天然水样品中弱酸可分解氰化物的测定结果与批次参考程序在95%置信水平下获得的结果一致。与连续添加试剂的流系统相比,分析功能得到了改善(灵敏度和采样率分别提高了90%和83%),OPA的消耗降低了230倍。

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